Lesson 4

Live your life. Create your destiny.

Department of Chemical, Metallurgical & Materials Engineering

Have u seen such before???
 Chapter 13: Particle Size Enlargement
13.1. Introduction
– Size enlargement: is the process by which smaller particles are
put together to form larger masses in which the original particles
can still be identified.
– Size enlargement is one of the single most important process steps
involving particulate solids in the process industries.

Industrial Applications of size enlargement:

• Pharmaceutical industry
• Agricultural industry
• Food industry
• Minerals industry
• Metallurgical industry
• Ceramics
The OBJECTIVE!!!!
Why particle size enlargement?
• Reduction of dust hazard (explosion hazard or health
hazard).
• To reduce caking and lump formation.
• To improve flow properties.
• To increase bulk density for storage.
• To provide a defined metered quantity of active
ingredient (e.g. pharmaceutical drug formulations).
• Control of surface to volume ratio (e.g. catalyst support).

Objectives of this lesson

– Inter-particle forces
– Growth mechanism
– Size enlargement processes
13.2. Inter-particle Forces
There are many inter-particle forces that exist, for the purpose of
this course we will only discuss the following six:

– van der Waals forces

– Forces due to adsorbed liquid layers
– Forces due to liquid bonding
– Electrostatic forces
– Solid bridges
– Comparison and interaction between forces
• van der Waals Forces

– There exist between all solids molecularly based attractive

forces collectively known as van der Waals forces.
– The energy of these forces is of the order of 0.1 eV and
decreases with the sixth power of the distance between
molecules.
– The range of van der Waals forces is large compared with that of
chemical bonds.
– The attractive force, FVW, between a sphere and a plane surface
as a result of van der Waals forces was derived by Hamaker
(1937) and is usually presented in the form:
KH R
FVW 
6 y2

– where KH is the Hamaker constant, R is the radius of the sphere

and y is the gap between the sphere and the plane.
• Forces due to Adsorbed Liquid Layers

– Particles in the presence of a condensable vapour will have a

layer of adsorbed vapour on their surface.
– If these particles are in contact a bounding forces results from
the overlapping of the adsorbed layers.
– The strength of the bond is dependent on the area of contact
and the tensile strength of the adsorbed layers.
– The thickness and strength of the layers increase with increasing
partial pressure of the vapour in the surrounding atmosphere.
• Forces due to Liquid Bonding

– Even in very small proportions, the presence of liquid on the

surface of particles affects the interparticle forces by the
smoothing effect it has on surface imperfections (increasing
particle-particle contact) and its effect of reducing the
interparticle distance.
– However, these forces are usually negligible in magnitude
compared with forces resulting when the proportion of liquid
present is sufficient to form interparticle liquid bridges.
– Newitt and Conway-Jones (1958) identified four types of liquid
states depending on the proportion of liquid present between
groups of particles:
• Pendular
• Funicular
• Capillary
• Droplet
 Pendular Funicular

droplet
capillary
Electrostatic Forces:

• Electrostatic charging of particles and surfaces occurs

as a result of friction caused by inter-particle collisions
and frequent rolling of particles against equipment
surfaces during processing.
• The charge is caused by the transfer electrons
between the bodies.
• The force between two charged spheres is proportional
to the product of their charges.
• Electrostatic forces may be attractive or repulsive, do
not require contact between particles and can act over
relatively long distances compared with adhesional
forces which require contact.
• Solid Bridges

– Granules formed by liquid bridges are usually not the end

product in a granulation process.
– More permanent bonding within the granule is created by solid
bridges formed as liquids removed from the original granule.
– Solid bridges between particles may take three forms:

• Crystalline bridges
• Liquid binder bridges
• Solid binder bridges

– If the material of the particles is soluble in the liquid added to

create granules, crystalline bridges may be formed when the
liquid evaporates.
– The process of evaporation reduces the proportion of
liquid in the granules producing high strength pendular
bridges before crystals form.

– Alternatively, the liquid used initially to form the granules

may contain a binder or glue which takes effect upon
evaporation of solvent.

– In some cases a solid binder may be used. This is a finely

ground solid which reacts with the liquid present to
produce a solid cement to hold the particles together.
• Comparison and Interaction between Forces

– In practice all inter-particle forces act simultaneously.

– The relative importantace of the forces varies with changes in
particle properties and with changes in the humidity of the
surrounding atmosphere.
– There is considerable interaction between the bonding forces.
– For example, in aqueous systems adsorbed moisture can
considerably increase van der Waals forces.
– Adsorbed moisture can also reduce inter-particle friction and
potential for interlocking, making the powder more free-flowing.
Electrostatic forces decay rapidly if the humidity of the
surrounding air is increased.
– A powder which in a dry atmosphere exhibits cohesivity due to
electrostatic humidity of the atmosphere is increased. If humidity
is further increased liquid bridge for motion can result in a return
to cohesive behaviour.
13.2. Growth Mechanism
There are essentially two types of processes that cause
agglomeration of particles when they are suspended in a fluid:

– Perikinetic process

– Orthokinetic process
• Perikinetic Processes

– Are attributable to Brownian movement can therefore

occur even in the in a static fluid.
– Double-layer repulsive forces and van der Waals
attractive forces may both operate independently in
disperse systems.
– Repulsion forces decrease exponentially with distance
across the ionic double-layer, although attraction forces
decrease, at larger distances from the particle surface,
and are inversely proportional to the distance.
– Consequently, attraction normally predominates both at
very large distances, and repulsion over intermediate
distances.
– Fine particles may also be held together by electrostatic
forces.
• Orthokinetic Processes

– Occur where the perikinetic process is supplemented by the

action of eddy currents which may be set up in stirred vessels
or in flowing systems.
– In these circumstances, the effects of the perikinetic mechanism
are generally negligible.

The change in agglomeration size as a function of time may be

represented by equation of the form:
d t3  A1  B1t (1)
For perikinetic:

dt
log  A2  B2t (2)
For orthokinetic: d0
where dt is the agglomerate size at time t. The
dimensions of A1 are L3, of B1 are L3T-1 and B2 are T-1.
A2 is dimensionless.

Equations (1) and (2) will apply only in the initial stages
of the enlargement process, since otherwise they
would indicate an indefinite increase of size dt with time
t.
Figure: Process stages of particle growth mechanism:
agglomeration
In general, starting with a mixture of particles of uniform size, the
following stages may be identified:

– Nucleation – fresh particles are formed, generally

by attrition.
– Layering or coating – as material is deposited on
the surfaces of the nuclei, thus increasing both the
size and total mass of the particles.
– Coalescence of particles – results in an increase
in particle size but not in the total mass of particles.
– Attrition – this results in degradation and formation
of small particles, thus generating nuclei that re-
enter the cycle again.
 What are Pellets:
• Pellets are free flowing spherical units prepared
from fine particle powder.
• Size- 0.5 to 1.5mm
• For oral drug delivery/control drug delivery.
• Coated pellets are administered in the form of soft
gelatin capsule or disintegrating tablet so that they
remove to content in gastric environments.
• Shows their flexibility in different formulations.
 Properties of Pellets:
• Excellent stability
• Dust free round pallets
• Good flow bahaviour
• easy to dose
• Compact structure
• Low Hygroscopicity
• High bulk density
• Dense uniform surface
• High active ingredient is possible
• Controlled release application
• Drug absorption can be altered
13.3. Size Enlargement Processes;
There are several processes commonly used for size enlargement:

– Spray drying
– Prilling
– Fluidized beds and Spouted beds
– Drum and pan agglomerators
– Pugs mills and extruders
– Elevated temperatures
– Pressure compaction
• SPRAY DRYING

– In this case, particle size is largely determined by the

size of the droplet of liquid or suspension, which may
be controlled by a suitably designed spray nozzle.
– The aggregates of dried material are held together as
a result of the deposition of small amount of solute on
the surface of the particles.
– For a given nozzle, the drop sizes will be a function of
both flowrate and liquid properties, particularly
viscosity, and to a lesser extent of outlet temperature.
– In general, viscous liquids tend to form large droplets
yielding large aggregate.
FLUIDIZED BED DRYER

1] Detachable
chamber
2] Fluidized bed
3] Fluidized gas &
liquid
4] Blower
5] Heater
6] Filter
7] Filter bag
Principle Operation:
• The bottom contains powder which we have to pelletize, is placed
in a detachable bowl.
• Two nozzles are there: (1)hot air and (2)binding agent
• Then it is pushed into dryer fresh air is allowed to pass through
filter which subsequently get heated into heater.
• Powder lifted from bottom and suspended in air the condition we
called fluidized state.
• the powder remain partially suspended in the gas stream, then the
granule rise in the container because of high velocity of gas (3-8
m/s)
• Fluidized state: the gas surrounding every forming pellets to
complete them dry & uniform.
• The air leaves dryer by passing through the filter. Process is
continued until desired size pellet is formed.
• DRUM AND PAN AGGLOMERATORS

– In drum agglomerators Particles are “tumbled” in an open

cylinder with roughened walls and subjected to a combination of
gravitational and centrifugal forces.
– In order to aid agglomeration, liquid may be sprayed on to the
surface of the bed or introduced through distribution pipes under
the bed.
– Mean retention times in the equipment are in the range 60 to
120s.
– In pan agglomerator, a classifying action may be achieved
which results in the fines having preferentially longer retention
time.
– Larger, denser and stronger agglomerates are produced
compared with those from the drum agglomerator.
 Rotating drums can be used in the
formation of slates, drying of liquid
feeds to coarse powders, and
flaking of resins, hot melt
adhesives, and other chemicals

Drum agglomerator
• Pressure Compaction

– If a material is subjected to very high compaction forces

it may be formed into sheets, briquettes or tablets.
– In the tableting machine used for producing pills of
pharmaceuticals, the powder is compressed into dies,
either with or without the addition of a binder.
– Powder compaction may also be achieved in roll
processes, including briquetting, in which compression
takes place between two rollers rotating at the same speed
– that is without producing any shearing action.
– In pellet mills, a moist feed is forced through die holes
where the resistance is attributable to the friction between
the powder and the walls of the dies.